CN207659359U - Uninanned platform equipment of the organic disulfide for pyrophosphate fire retardant - Google Patents
Uninanned platform equipment of the organic disulfide for pyrophosphate fire retardant Download PDFInfo
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- CN207659359U CN207659359U CN201721424117.8U CN201721424117U CN207659359U CN 207659359 U CN207659359 U CN 207659359U CN 201721424117 U CN201721424117 U CN 201721424117U CN 207659359 U CN207659359 U CN 207659359U
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- reaction kettle
- circulating slot
- diluted alkaline
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Abstract
The utility model provides a kind of uninanned platform equipment of organic disulfide for pyrophosphate fire retardant; contain the reaction kettle for acylation reaction and esterification; the reaction kettle has neopentyl glycol entrance, phosphorus thiochloride entrance, technique water inlet, offgas outlet, or also pyridine entrance；Condenser, jet pump are sequentially connected after the tail gas gas outlet of the reaction kettle, diluted alkaline circulating slot is interconnected with jet pump and being capable of circularly absorbing hydrogen chloride tail gas.The utility model has saved consumption of raw materials cost, reduces impurity, and the rate of recovery of pyridine is higher.
Description
Technical field
The utility model belongs to the technology of preparing of phosphonium flame retardant.
Background technology
In traditional chemical reaction, solvent is most common reaction medium, because they can be molten by reactant well
Solution forms homogeneous system, and reaction is made to be smoothed out.
Early in the thirties in last century, fire-proof flame-retarded agent has started to be applied in the flame retardant treatment of cellulose fibre, this
A little fire retardants are mainly fabric post-treatment fire retardant, easy to use, but the additive amounts such as solvent are more, and influence performance, are increased
Addition sheet, flame retardant effect cannot be lasting.Such as：
The first phase in 2010,《Chemical Engineer》" synthesis of the double neopentyl glycol ester fire retardants of two thio pyrophosphoric acids and table
Sign ", using neopentyl glycol and phosphorus thiochloride as raw material, dimethylbenzene is solvent, and P has been synthesized under the action of pyridine and triethylamine,
Double neopentyl glycol ester (the B G D llP) fire retardants of one or two thio pyrophosphoric acids of P '.
Application number：2009801414849 prepare method of the organic disulfide for pyrophosphate, the two-stage process having, and use
3- picolines are used as solvent and alkali simultaneously, from corresponding 1,3- glycol and thiophosphoryl chloride prepare wherein R1, R2, R3, R4 and
R5 independently is the organic disulfide of the formula (I) of hydrogen, C1-4 alkyl, chloromethyl or bromomethyl for pyrophosphate.
Invention content
Purpose of utility model：It provides a kind of fire-retardant for pyrophosphate without using solvent, the organic disulfide cut down the consumption of raw materials
The uninanned platform technique and equipment of agent.
To achieve the above object, technical scheme is as follows：
The organic disulfide of the utility model for pyrophosphate, is used using neopentyl glycol and phosphorus thiochloride as primary raw material
Reaction kettle first passes through the acylation reaction stage, using esterification stage.
（1）The acylation reaction stage does not add any solvent.Specific steps：A small amount of neopentyl glycol paving is first put into reaction kettle
Bottom is warming up to 50 DEG C or so and plays dissolution assistant effect（The RAW MATERIALS Neopentyl glycol to heat up on a small quantity not only one of the raw material as reaction, but also tool
There is the miscible formation homogeneous system of raw materials such as similar solvent help and the phosphorus thiochloride being added afterwards, thus without using other
Solvent；Temperature is only used as solvent function, participates in chemically reacting again after heating at this time less than the temperature that chemical reaction needs simultaneously）.
Then, phosphorus thiochloride is added dropwise while remaining neopentyl glycol being put into reaction kettle；Then, reaction system is warming up to 85 ~ 95
℃（The reasons why temperature is set：The yield of fire retardant is higher under this temperature condition）Acylation reaction is carried out, acid binding agent pyrrole is added
Pyridine, accelerates the speed of acylation reaction, and prevents the generation of kelene.
（2）There is by-product hydrogen chloride generation during acylation reaction, is -1 by the pressure in tail gas regulating valve control reaction kettle
~-3KPa（Due to thering is by-product hydrogen chloride gas generation, control negative pressure on the one hand to prevent reaction kettle superpressure, another party in reaction process
Face promotes reaction to be carried out to forward direction）；Work as hypertonia（＞ -1KPa）When, increase tail gas control valve opening；Work as hypotony（＜-
3KPa）, reduce tail gas controlling opening of valve.
（3）Process water is added when being reduced to 80 DEG C or so after acylation reaction, at a temperature of reaction system, be esterified anti-
It answers, until the rate of collecting of neopentyl glycol reaches 80% or more（This temperature ensures that esterification quickly carries out, which can sentence
Other fire retardant has very in high yield）, organic disulfide is obtained for pyrophosphate fire retardant.
Acylated stage solventless method technique saves the processing step that solvent is used and recycled compared with colleague, had both reduced raw material and has disappeared
Cost is consumed, and avoids introducing solvent impurity into acid binding agent pyridine, the rate of recovery of the acid binding agent pyridine in later stage is higher.
The reaction kettle has neopentyl glycol entrance, phosphorus thiochloride entrance, technique water inlet, offgas outlet, or also
There is pyridine entrance.Condenser, jet pump, diluted alkaline circulating slot and injection are sequentially connected after the tail gas gas outlet of the reaction kettle
Pump connection and mutual unicom, ensure lye circularly absorbing hydrogen chloride tail gas；Separately it is furnished with alkali storage tank, alkali storage tank and diluted alkaline circulating slot phase
Connection, to supplement the lye wherein consumed.
Pass through the condensation of condenser so that the gaseous raw material in part and pyridine condensing reflux reduce consumption of raw materials.Than
Purer hydrogen chloride emits, then by dilute in the collective effect of jet pump and diluted alkaline circulating slot, with diluted alkaline circulating slot
Lye carries out neutralization reaction recycling.
It is connected with supply pump machine between diluted alkaline circulating slot and alkali storage tank, pH meter, pH meter and benefit are installed in diluted alkaline circulating slot
Chain adjusting relationship is formed to pump machine.When pH value is down to 7, pump machine is automatically turned on mends alkali into diluted alkaline slot, when pH value is to 12,
Pump machine is chain voluntarily to close.
Tail gas is absorbed using jet pump, is reduced to the operating personnel's injury that feeds intake, corrosion of the reduction to field device.
Advantageous effect：
The utility model proposes this solventless method technique, be greatly saved consumption of raw materials and plus solvent consumption at
This；The step of solvent is used and recycled is saved, system impurity is reduced, the rate of recovery of pyridine is higher；Exhaust system automatic control technique can
The acylated system pressure of serialization control, pressure and tail gas regulating valve are chain, and on-line analysis diluted alkaline circulating slot pH simultaneously realizes automatic mend
Alkali promotes live the degree of automation, reduces employee work amount.
Description of the drawings
Fig. 1 is a kind of device structure schematic diagram of utility model：
In figure, 1- reaction kettles, 2- phosphorus thiochlorides entrance, 3- neopentyl glycols entrance, 4- offgas outlets, 5- condensers, 6- tails
Gas control valve, 7- jet pumps, 8- diluted alkalines circulating slot, 9-pH meters, 10- alkali storage tanks.
Specific implementation mode
Organic disulfide as shown in Figure 1 has reaction kettle, with new penta for the uninanned platform equipment of pyrophosphate fire retardant
Glycol and phosphorus thiochloride are primary raw material, and there is the reaction kettle neopentyl glycol entrance, phosphorus thiochloride entrance, process water to enter
Mouth, offgas outlet, or also pyridine entrance；It is sequentially connected condenser, jet pump, diluted alkaline after the tail gas gas outlet of reaction kettle
Circulating slot is connect with jet pump and mutual unicom circularly absorbing hydrogen chloride tail gas.
Separately it is furnished with alkali storage tank, alkali storage tank is connected with diluted alkaline circulating slot, to supplement the lye wherein consumed.Diluted alkaline circulating slot
It is connected with supply pump machine between alkali storage tank, pH meter is installed in diluted alkaline circulating slot, pH meter forms chain adjusting with supply pump machine
Relationship.
Claims (3)
1. a kind of organic disulfide is for the uninanned platform equipment of pyrophosphate fire retardant, containing for acylation reaction and esterification
Reaction kettle, it is characterised in that：
The reaction kettle has neopentyl glycol entrance, phosphorus thiochloride entrance, technique water inlet, offgas outlet, or also pyrrole
Pyridine entrance；It is sequentially connected condenser, jet pump, diluted alkaline circulating slot and jet pump phase after the tail gas gas outlet of the reaction kettle
It is intercommunicated so as to circularly absorbing hydrogen chloride tail gas.
2. synthesis device as described in claim 1, it is characterised in that：Separately it is furnished with alkali storage tank, alkali storage tank and diluted alkaline circulating slot phase
Connection.
3. synthesis device as described in claim 1, it is characterised in that：It is connected with replenishment pump between diluted alkaline circulating slot and alkali storage tank
Machine, pH meter is equipped in diluted alkaline circulating slot, and pH meter forms chain adjusting relationship with supply pump machine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721424117.8U CN207659359U (en) | 2017-10-31 | 2017-10-31 | Uninanned platform equipment of the organic disulfide for pyrophosphate fire retardant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721424117.8U CN207659359U (en) | 2017-10-31 | 2017-10-31 | Uninanned platform equipment of the organic disulfide for pyrophosphate fire retardant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN207659359U true CN207659359U (en) | 2018-07-27 |
Family
ID=62937636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201721424117.8U Active CN207659359U (en) | 2017-10-31 | 2017-10-31 | Uninanned platform equipment of the organic disulfide for pyrophosphate fire retardant |
Country Status (1)
| Country | Link |
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| CN (1) | CN207659359U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674096A (en) * | 2017-10-31 | 2018-02-09 | 南通江山农药化工股份有限公司 | Uninanned platform technique and its equipment of the organic disulfide for pyrophosphate fire retardant |
| CN109675514A (en) * | 2019-01-04 | 2019-04-26 | 南京工业大学 | A kind of preparation facilities of the packaging fire retardant of superficial layer |
| CN109705390A (en) * | 2018-12-29 | 2019-05-03 | 南京师范大学 | A kind of Halogen ring-type pyrophosphate is preparing the application in flame retarded rigid polyurethane foams plastics |
-
2017
- 2017-10-31 CN CN201721424117.8U patent/CN207659359U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674096A (en) * | 2017-10-31 | 2018-02-09 | 南通江山农药化工股份有限公司 | Uninanned platform technique and its equipment of the organic disulfide for pyrophosphate fire retardant |
| CN109705390A (en) * | 2018-12-29 | 2019-05-03 | 南京师范大学 | A kind of Halogen ring-type pyrophosphate is preparing the application in flame retarded rigid polyurethane foams plastics |
| CN109675514A (en) * | 2019-01-04 | 2019-04-26 | 南京工业大学 | A kind of preparation facilities of the packaging fire retardant of superficial layer |
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